Darstellung und Kristallstruktur eines Semiammoniakates von Natriumtetraamidozinkat, Na2Zn(NH2)4 · 0,5 NH3

In this contribution, first synthesis of semiconducting ZnSiN 2 and ZnGeN 2 from solution is reported with supercritical ammonia as solvent and KNH 2 as ammonobasic mineralizer.T he reactions were conducted in custom-built highpressure autoclaves made of nickel-based superalloy.T he nitrides were characterized by powder X-ray diffractiona nd their crystal structures were refinedb yt he Rietveld method. ZnSiN 2 (a = 5.24637(4), b = 6.28025(5), c = 5.02228(4) , Z = 4, R wp = 0.0556) and isotypic ZnGeN 2 (a = 5.46677(10), b = 6.44640(12), c = 5.19080(10) , Z = 4, R wp = 0.0494) crystallize in the orthorhombic space group Pna2 1 (no. 33). The morphology and elemental composition of the nitrides were examined by electron microscopy and energy-dispersive X-ray spectroscopy (EDX). Well-definedsingle crystalswith adiameter up to 7 mmw ere grownb ya mmonothermal synthesis at temperatures between 870 and 1070 Ka nd pressures up to 230 MPa. Optical properties have been analyzed with diffuse reflectance measurements. The band gaps of ZnSiN 2 and ZnGeN 2 were determined to be 3.7 and 3.2 eV at room temperature, respectively.I ns itu X-ray measurements were performed to exemplarily investigate the crystallization mechanism of ZnGeN 2 .D issolution in ammonobasic supercritical ammonia between 570 and6 70 Kw as observed which is quite promising for the crystal growth of ternary nitrides under ammonothermalconditions.

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Ammonothermal Synthesis of Earth‐Abundant Nitride Semiconductors ZnSiN₂ and ZnGeN₂ and Dissolution Monitoring by In Situ X‐ray Imaging

Häusler

Schimmel

Wellmann

et al. 2017

Chemistry A European J

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ChemInform Abstract: Synthesis and Crystal Structure of a Semiammoniate of Sodium Tetraamidozincate, Na₂Zn(NH₂)₄×0.5NH₃.

Froehling

Jacobs

1998

ChemInform

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structure structure (solids and liquids) D 2000 -018Synthesis and Crystal Structure of a Semiammoniate of Sodium Tetraamidozincate, Na 2 Zn(NH 2 ) 4 ·0.5NH 3 .-Single crystals of the title compound are obtained in the attempt to synthesize Na 2 Zn(NH 2 ) 4 from the corresponding metals in liq. NH 3 at room temp. (autoclave, 12 d). Na 2 Zn(NH 2 ) 4 ·0.5NH 3 crystallizes in the space group C2/c with Z = 24. The structure contains isolated molecular [Zn(NH 2 ) 4 ] 2− ions connected by Na + ions. The N atoms are distorted hexagonally close packed with Zn 2+ and Na + occupying the tetrahedral and octahedral sites, respectively.

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Ammonothermal Synthesis and Characterization of First Amidozincate Hydroxides

et al. 2021

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The first alkali metal amidozincate hydroxides Na 3 [Zn(NH 2 ) 4 ](OH) and Na 3 [Zn(NH 2 ) 3 ](OH) 2 were obtained from supercritical ammonia under ammonobasic conditions at 823 K and 250 MPa, and 623 K and 159 MPa, respectively. Crystal structures have been refined against single crystal X-ray diffraction intensity data. Coordination environments of the cations as well as the rather open crystal structure and low density of Na 3 [Zn(NH 2 ) 4 ](OH) suggest the initial formation of a monoammoniate, prior loss of ammonia during depressurizing and recovery of the product.While Na 3 [Zn(NH 2 ) 4 ](OH) contains mutually isolated amidozincate ions next to hydroxide ions, Na 3 [Zn(NH 2 ) 3 ](OH) 2 is the first amidozincate realizing a condensation of the complex anionic substructure so far. Both compounds are regarded possible intermediates in an ammonothermal zinc nitride synthesis and give insights into the action of impurities during ammonothermal processes. Raman spectroscopic measurements support the assignment of amide and hydroxide groups.

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Darstellung und Kristallstruktur eines Semiammoniakates von Natriumtetraamidozinkat, Na2Zn(NH2)4 · 0,5 NH3

Cited by 7 publications

References 6 publications

Ammonothermal Synthesis of Earth‐Abundant Nitride Semiconductors ZnSiN₂ and ZnGeN₂ and Dissolution Monitoring by In Situ X‐ray Imaging

Ammonothermal Synthesis of Earth‐Abundant Nitride Semiconductors ZnSiN₂ and ZnGeN₂ and Dissolution Monitoring by In Situ X‐ray Imaging

ChemInform Abstract: Synthesis and Crystal Structure of a Semiammoniate of Sodium Tetraamidozincate, Na₂Zn(NH₂)₄×0.5NH₃.

Ammonothermal Synthesis and Characterization of First Amidozincate Hydroxides

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Darstellung und Kristallstruktur eines Semiammoniakates von Natriumtetraamidozinkat, Na2Zn(NH2)4 · 0,5 NH3

Cited by 7 publications

References 6 publications

Ammonothermal Synthesis of Earth‐Abundant Nitride Semiconductors ZnSiN2 and ZnGeN2 and Dissolution Monitoring by In Situ X‐ray Imaging

Ammonothermal Synthesis of Earth‐Abundant Nitride Semiconductors ZnSiN2 and ZnGeN2 and Dissolution Monitoring by In Situ X‐ray Imaging

ChemInform Abstract: Synthesis and Crystal Structure of a Semiammoniate of Sodium Tetraamidozincate, Na2Zn(NH2)4×0.5NH3.

Ammonothermal Synthesis and Characterization of First Amidozincate Hydroxides

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Product

Resources

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Ammonothermal Synthesis of Earth‐Abundant Nitride Semiconductors ZnSiN₂ and ZnGeN₂ and Dissolution Monitoring by In Situ X‐ray Imaging

Ammonothermal Synthesis of Earth‐Abundant Nitride Semiconductors ZnSiN₂ and ZnGeN₂ and Dissolution Monitoring by In Situ X‐ray Imaging

ChemInform Abstract: Synthesis and Crystal Structure of a Semiammoniate of Sodium Tetraamidozincate, Na₂Zn(NH₂)₄×0.5NH₃.